CN109735846B - Deplating liquid, preparation method and application thereof - Google Patents
Deplating liquid, preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a deplating solution, a preparation method and application thereof. The deplating solution comprises the following components in percentage by mass: 5 to 10 percent of oxidant, 1 to 5 percent of corrosion inhibitor, 1 to 2 percent of brightener, 1 to 5 percent of dissolution accelerator, 10 to 15 percent of accelerator, 1 to 5 percent of activator and water; the oxidant is nitric acid; the corrosion inhibitor is a phenol compound; the brightener is polyvinylpyrrolidone with K value less than 20; the cosolvent is a chlorine-containing compound; the accelerator is sulfamic acid and/or citric acid. The deplating liquid has the advantages of wide application range, high deplating speed, low corrosion rate to base materials, no precipitate, good stability, low yellow smoke generation amount, low nitric acid consumption and low loss rate, and has very wide market application prospect.
Description
Technical Field
The invention relates to a deplating solution, a preparation method and application thereof.
Background
The electroplating tin stripping liquid used after semiconductor packaging currently has a sulfuric acid-hydrogen peroxide system and a nitric acid system, wherein the nitric acid system is more stable and efficient, and is more widely applied than the sulfuric acid-hydrogen peroxide system. Most of the existing deplating solutions of nitric acid systems have high nitric acid content and generate a large amount of yellow smoke in the using process. The nitric acid system deplating solution is developed towards low nitric acid and low yellow smoke at present.
Patent CN105297122B mentions a special stripping solution for an automatic electroplating production line of electronic components. The content of nitric acid in the invention is higher than 15-35 parts, the problem of yellow smoke is not solved, and the metal of the tin-plated base material of the electronic component is not disclosed.
Patent CN105821411A mentions a chemical stripping solution for semiconductor process and a preparation method thereof. The deplating solution comprises nitric acid, ferric nitrate, methanesulfonic acid, a corrosion inhibitor and deionized water, and can also comprise a nitric acid stabilizer, but specific components of the nitric acid stabilizer are not disclosed, and the effect of solving the problem of nitric acid stability in the deplating process is not obvious under the condition that the nitric acid stabilizer is not contained.
Therefore, it is highly desirable to develop a deplating solution with wide applicability, fast deplating speed, no precipitation, no corrosion to the substrate, low nitric acid consumption, low nitric acid loss rate and low yellow smoke.
Disclosure of Invention
The invention aims to solve the technical problems that the existing stripping solution has high nitric acid content and unsatisfactory stability, generates a large amount of yellow smoke in the use process and the like, and provides the stripping solution, a preparation method and application thereof. The deplating liquid has the advantages of wide application range, high deplating speed, low corrosion rate to base materials, no precipitate, good stability, low yellow smoke generation amount, low nitric acid consumption and low loss rate, and has very wide market application prospect.
The invention mainly solves the technical problems through the following technical means:
the invention provides a deplating solution which comprises the following components in percentage by mass: 5 to 10 percent of oxidant, 1 to 5 percent of corrosion inhibitor, 1 to 2 percent of brightener, 1 to 5 percent of dissolution accelerator, 10 to 15 percent of accelerator, 1 to 5 percent of activator and water;
the oxidant is nitric acid; the corrosion inhibitor is a phenol compound; the brightener is polyvinylpyrrolidone with a K value of less than 20; the cosolvent is a chlorine-containing compound; the accelerator is sulfamic acid and/or citric acid.
In the present invention, the mass fraction of the oxidizing agent is preferably 6% to 8%, more preferably 6.5% to 7.5%. The mass fraction of the corrosion inhibitor is preferably 2% -4%, more preferably 2.5% -3.5%. The mass fraction of the brightener is preferably 1.2% -1.8%, more preferably 1.5% -1.6%. The mass fraction of the dissolution promoter is preferably 2% -4%, more preferably 3% -3.5%. The mass fraction of the accelerator is preferably 12% to 14%, more preferably 13% to 13.5%. The mass fraction of the activating agent is preferably 2.5-4.5%, more preferably 3-3.5%.
In the deplating solution, the sum of the mass fractions of the components is 100%, so the water is preferably used in an amount of 100% for complementing the sum of the mass fractions of the components.
The phenolic compound is preferably catechol and/or pyrogallol.
The brightener is preferably polyvinylpyrrolidone with K less than 20 and not more than 12, and is more preferably one or more of polyvinylpyrrolidone with K values of 12, 15 and 17.
The chlorine-containing compound is preferably potassium chloride and/or sodium chloride.
The activating agent may be an activating agent conventionally used in the art, preferably sodium nitrite and/or sodium hypochlorite.
The water is preferably one or more of deionized water, distilled water, pure water and ultrapure water.
In a preferred embodiment of the present invention, the deplating solution comprises the following components by mass: 5 to 10 percent of oxidant, 1 to 5 percent of corrosion inhibitor, 1 to 2 percent of brightener, 1 to 5 percent of dissolution accelerator, 10 to 15 percent of accelerator, 1 to 5 percent of activator and water; the oxidant is nitric acid; the corrosion inhibitor is a phenol compound; the brightener is polyvinylpyrrolidone with a K value of less than 20; the cosolvent is a chlorine-containing compound; the accelerator is sulfamic acid and/or citric acid.
In a preferred embodiment of the present invention, the deplating solution comprises the following components by mass: 6 to 8 percent of oxidant, 2 to 4 percent of corrosion inhibitor, 1.2 to 1.8 percent of brightener, 2 to 4 percent of dissolution promoter, 12 to 14 percent of accelerator, 2.5 to 4.5 percent of activator and water; the oxidant is nitric acid; the corrosion inhibitor is a phenol compound; the brightener is polyvinylpyrrolidone with a K value of less than 20; the cosolvent is a chlorine-containing compound; the accelerator is sulfamic acid and/or citric acid.
In a preferred embodiment of the present invention, the deplating solution comprises the following components by mass: 6.5 to 7.5 percent of oxidant, 2.5 to 3.5 percent of corrosion inhibitor, 1.5 to 1.6 percent of brightener, 3 to 3.5 percent of dissolution accelerator, 13 to 13.5 percent of accelerator, 3 to 3.5 percent of activator and water; the oxidant is nitric acid; the corrosion inhibitor is a phenol compound; the brightener is polyvinylpyrrolidone with a K value of less than 20; the cosolvent is a chlorine-containing compound; the accelerator is sulfamic acid and/or citric acid.
The invention also provides a preparation method of the deplating solution, which comprises the following steps: and mixing the components of the deplating solution.
The invention also provides application of the deplating solution in deplating the tinned substrate.
The tin-plated substrate is preferably a tin-plated copper substrate or a tin-plated iron-nickel substrate.
Said application preferably comprises the following steps: and (3) contacting the tinning substrate with the deplating solution to deplate. More preferably comprising the steps of: and (3) contacting the tinned substrate with the deplating solution for deplating, cleaning and drying.
Wherein the temperature of the contact deplating can be 20-60 ℃, and preferably 40-45 ℃.
The washing operation and conditions may be those conventional in the art, and preferably washing with water.
The drying operation and conditions may be those conventional in the art, and are preferably blow-dried with nitrogen.
The above preferred conditions can be arbitrarily combined to obtain preferred embodiments of the present invention without departing from the common general knowledge in the art.
The reagents and starting materials used in the present invention are commercially available.
The positive progress effects of the invention are as follows: the deplating liquid prepared by the preparation method has the advantages of high deplating speed, low corrosion rate to a base material, wide application range, high saturated tin dissolution, no precipitation and good stability; the method has the advantages of low consumption of nitric acid serving as an oxidant, low loss rate of nitric acid in the deplating process, low generation amount of yellow smoke and wide market application prospect.
Detailed Description
The invention is further illustrated by the following examples, which are not intended to limit the scope of the invention. The experimental methods without specifying specific conditions in the following examples were selected according to the conventional methods and conditions, or according to the commercial instructions.
In the following examples and comparative examples, the method for preparing the deplating solution includes the following steps of mixing the components of the deplating solution.
Examples 1 to 11
TABLE 1 stripping liquid Components
TABLE 2 Mass fractions of the components
Comparative examples 1 to 12
TABLE 3 Components of deplating solutions
TABLE 4 mass fraction of each component
Among them, comparative examples 1-2 explore the effect of using an accelerator other than sulfamic acid and citric acid as an accelerator; in comparative examples 3 to 7, the effect of using polyvinylpyrrolidone with K being more than or equal to 20 as the brightener is explored; the effects of using other salts than the chlorine-containing compound as the solubilizing agents were explored in comparative examples 8 to 11; in comparative example 12, the effect of using a corrosion inhibitor other than phenol compounds as a corrosion inhibitor was investigated.
Effects of the embodiment
And (3) stripping effect testing:
the size of the particles is 6 x 6cm2And the tin-plated copper base material with the tin layer of 5 mu m is soaked in 1L of deplating solution, the tin-plated copper base material and the deplating solution are contacted for deplating, the temperature for contact deplating is 40 ℃, and the time required for observing the copper layer to be completely exposed is required. And fishing out the copper substrate after the copper layer is completely exposed, cleaning with water and drying with nitrogen. The time taken for the copper layer to be completely exposed is the deplating completion time.
Testing the corrosion rate of the base material:
non-tinned 6X 6cm2The copper base material or the iron-nickel base material is soaked in 1L of deplating solution for 1h at the temperature of 40 ℃, and is cleaned by water and dried by nitrogen after soaking. And calculating the corrosion amount of the copper base material or the iron-nickel base material before and after soaking by a weighing method, wherein the corrosion amount is divided by the soaking time to obtain the corrosion rate.
A nitric acid month loss rate testing step:
and standing the deplating solution for 30 days at 40 ℃, and measuring the acidity of the nitric acid by adopting an acid-base titration method to measure the monthly loss rate of the effective concentration of the nitric acid.
And (3) testing the saturated tin dissolving amount:
and (3) soaking the tin sheet with the purity of 98% in 1L of deplating solution at the soaking temperature of 40 ℃ until the mass of the tin sheet does not change any more, cleaning with water, drying with nitrogen, and calculating the mass change of the tin sheet before and after soaking by using a weighing method.
Testing the on-line application effect:
and (4) respectively using stripping solutions on the production lines of the tin-plated iron-nickel substrate and the tin-plated copper substrate, and observing the generation condition of precipitation in the stripping solutions and the corrosion condition of a production line pendant within one month.
The results of the various tests are shown in Table 5.
TABLE 5
As is apparent from the above-mentioned effect examples 1 to 11 and comparative effect examples 1 to 12, the stripping solution of the present invention has a low loss rate of nitric acid as an oxidizing agent, a high stripping rate, a low corrosion rate to a base material in a tin-plated base material, and a high saturated dissolved tin content, as compared with the stripping solution of the comparative example. The deplating liquid used in the invention has no precipitation in the application of the production line within one month, and has no obvious corrosion to the pendant of the production line.
As can be seen from comparative effect examples 1-2, when the accelerator was replaced with methanesulfonic acid or nitrilotriacetic acid, the monthly loss of nitric acid was high. It can be seen from comparative examples 3-7 that when the brightener was replaced with polyvinylpyrrolidone having a K of not less than 20, the deplating time of the same tin-plated copper base material was significantly prolonged, it was difficult to meet the industrial demand, the rate of nitric acid loss was high, and the saturated tin dissolution was also significantly reduced. As can be seen from comparative examples 8 to 11, when the dissolution accelerator was replaced with ferric nitrate, zinc sulfate, sodium acetate or ammonium fluoride, the stability of the deplating solution was deteriorated and precipitation occurred within one month upon application to the production line. As can be seen from the comparative example 12, when the corrosion inhibitor is replaced by benzotriazole, the corrosion rate to the copper base material and the iron-nickel base material is high, so that the base material loss is overlarge, and when the corrosion inhibitor is applied to a production line, a production line pendant is corroded.
Claims (14)
1. The deplating solution is characterized by comprising the following components in percentage by mass: 5 to 10 percent of oxidant, 1 to 5 percent of corrosion inhibitor, 1 to 2 percent of brightener, 1 to 5 percent of dissolution accelerator, 10 to 15 percent of accelerator, 1 to 5 percent of activator and water;
the oxidant is nitric acid; the corrosion inhibitor is a phenol compound; the brightener is polyvinylpyrrolidone with a K value of less than 20; the cosolvent is a chlorine-containing compound; the accelerator is sulfamic acid and/or citric acid.
2. The deplating solution according to claim 1, wherein the mass fraction of the oxidizing agent is 6-8%;
and/or the mass fraction of the corrosion inhibitor is 2-4%;
and/or the mass fraction of the brightener is 1.2-1.8%;
and/or the mass fraction of the cosolvent is 2-4%;
and/or the mass fraction of the accelerator is 12-14%;
and/or the mass fraction of the activating agent is 2.5-4.5%.
3. The deplating solution according to claim 2, wherein the mass fraction of the oxidizing agent is 6.5 to 7.5 percent;
and/or the mass fraction of the corrosion inhibitor is 2.5-3.5%;
and/or the mass fraction of the brightener is 1.5-1.6%;
and/or the mass fraction of the cosolvent is 3-3.5%;
and/or the mass fraction of the accelerator is 13-13.5%;
and/or the mass fraction of the activating agent is 3-3.5%.
4. The deplating solution according to claim 1 wherein said phenolic compound is catechol and/or pyrogallol;
and/or the brightener is polyvinylpyrrolidone with K less than 20 and more than or equal to 12;
and/or, the chlorine-containing compound is potassium chloride and/or sodium chloride;
and/or the activating agent is sodium nitrite and/or sodium hypochlorite;
and/or the water is one or more of deionized water, distilled water, pure water and ultrapure water.
5. The deplating solution according to claim 4 wherein said brightener is one or more of polyvinylpyrrolidone having K values of 12, 15 and 17.
6. The deplating solution according to claim 1, which consists of the following components in percentage by mass: 5 to 10 percent of oxidant, 1 to 5 percent of corrosion inhibitor, 1 to 2 percent of brightener, 1 to 5 percent of dissolution accelerator, 10 to 15 percent of accelerator, 1 to 5 percent of activator and water; the oxidant is nitric acid; the corrosion inhibitor is a phenol compound; the brightener is polyvinylpyrrolidone with a K value of less than 20; the cosolvent is a chlorine-containing compound; the accelerator is sulfamic acid and/or citric acid.
7. The deplating solution according to claim 1, which consists of the following components in percentage by mass: 6 to 8 percent of oxidant, 2 to 4 percent of corrosion inhibitor, 1.2 to 1.8 percent of brightener, 2 to 4 percent of dissolution promoter, 12 to 14 percent of accelerator, 2.5 to 4.5 percent of activator and water; the oxidant is nitric acid; the corrosion inhibitor is a phenol compound; the brightener is polyvinylpyrrolidone with a K value of less than 20; the cosolvent is a chlorine-containing compound; the accelerator is sulfamic acid and/or citric acid.
8. The deplating solution according to claim 1, which consists of the following components in percentage by mass: 6.5 to 7.5 percent of oxidant, 2.5 to 3.5 percent of corrosion inhibitor, 1.5 to 1.6 percent of brightener, 3 to 3.5 percent of dissolution accelerator, 13 to 13.5 percent of accelerator, 3 to 3.5 percent of activator and water; the oxidant is nitric acid; the corrosion inhibitor is a phenol compound; the brightener is polyvinylpyrrolidone with a K value of less than 20; the cosolvent is a chlorine-containing compound; the accelerator is sulfamic acid and/or citric acid.
9. A method for preparing the deplating solution according to any one of claims 1 to 8, comprising the following steps: and mixing the components of the deplating solution.
10. Use of a deplating solution according to any one of claims 1 to 8 for deplating a tin-plated substrate.
11. The use according to claim 10, wherein the tin-plated substrate is a tin-copper-plated substrate or a tin-iron-nickel-plated substrate;
and/or, the application comprises the following steps: and (3) contacting the tinning substrate with the deplating solution to deplate.
12. The use according to claim 11, characterized in that said use comprises the following steps: and (3) contacting the tinned substrate with the deplating solution for deplating, cleaning and drying.
13. The use according to claim 12, wherein the contact deplating temperature is from 20 ℃ to 60 ℃;
and/or, the cleaning is cleaning with water;
and/or the drying is blow-drying by nitrogen.
14. The use according to claim 13, wherein the contact deplating temperature is from 40 ℃ to 45 ℃.
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| CN112410792B (en) * | 2019-10-08 | 2023-03-31 | 叶涛 | PCB iron-free nitric acid type tin stripping water and regeneration and reuse method thereof |
| CN113122859A (en) * | 2021-04-21 | 2021-07-16 | 广东富行洗涤剂科技有限公司 | Stripping solution and process for lanthanum titanate tool in optical glass coating process |
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